反应 #155724

反应方程式

n-butyl bromide

Intermediate c

2-phenyl-3,5-dioxo-2,3,4,5-tetrahydro-1,2,4-triazine-6-carbonitrile

DMF

NaH

→

Intermediate f

收率 81.4%

2-phenyl-4-butyl-3,5-dioxo-2,3,4,5-tetrahydro-1,2,4-triazine-6-carbonitrile

收率 81.4%

溶剂

water

反应条件

后处理

1. 1
   workup.ADDITIONAfter the dropwise addition
2. 2
   workup.WAITthe reaction was conducted at 70° C. for 6 h
3. 3
   其他After completion of the reaction
4. 4
   其他A great deal of solid separated out
5. 5
   过滤was filtered by suction
6. 6
   洗涤The filtered cake was washed with water
7. 7
   其他dried

实验过程

Intermediate c (9 g, 0.042 mol) was added to DMF (100 mL). To the mixture was added NaH (1.3 g, 0.054 mol) in batch under an ice bath. After stirring for 30 min, n-butyl bromide (3.4 mL, 0.042 mol) was added dropwise. After the dropwise addition, the reaction was conducted at 70° C. for 6 h. After completion of the reaction, the reaction solution was poured into water (600 mL). A great deal of solid separated out and was filtered by suction. The filtered cake was washed with water and dried to produce Intermediate f (8.2 g) in a yield of 81.4%.

来源